HRID638331

反应详情

EQUATION

反应方程式

HRID 638331 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The above intermediate 2-(4-methoxyphenyl)-4-pyrimideneamine was prepared as follows: A slurry containing 81 g of 4-methoxybenzamidine hydrochloride, 24 g of sodium methoxide and 200 ml of methanol was stirred for 15 minutes, filtered and the filtrate concentrated in vacuo on a steam bath. To the residue was added β-ethoxyacrylonitrile (same as ethoxymethyleneacetonitrile) and the solution was heated at 100°-115° C. for 2 and 1/2 hours and poured into water. The solid was collected, washed with water, air-dried, and crystallized from ether-n-hexane to yield 85 g of 2-(4-methoxyphenyl)-4-pyrimidinamine, m.p. 102°-104° C.

WORKUP

后处理

  1. customThe above intermediate 2-(4-methoxyphenyl)-4-pyrimideneamine was prepared
  2. filtrationfiltered
  3. concentrationthe filtrate concentrated in vacuo on a steam bath
  4. additionTo the residue was added β-ethoxyacrylonitrile (same as ethoxymethyleneacetonitrile)
  5. temperaturethe solution was heated at 100°-115° C. for 2 and 1/2 hours
  6. additionpoured into water
  7. customThe solid was collected
  8. washwashed with water
  9. customair-dried
  10. customcrystallized from ether-n-hexane